Process for increasing the wetting capacity of alkaline treatment liquids



FRIEDRICH rosrmcn, or nImsnn rozr'r & comrANY, xoImANm'r ensnnnscrmrr,

Patented July 1 1, 1933 UNITED STATES PATENT OFFICE GERMANY, ASSIGNOR TO CHEMISGHE FABBJI OF DRESDEN, GERMANY rnocrss F013. INCREASING 'rnn wnrrINe CAPACITY or ALKALINE TREATMENT LIoUIns' No Drawing. Application filed March 16, 1931, Serial No. 523,174, and

I have filed applications in Germany (a) March 14, 1930, (1)) March 15, 1930, (0) March 17', 1930.- v

This invention relates to a process of increasing the wetting action of alkaline treatment liquids for textile material, and to the treatment baths thus produced. More particularly my invention relates to such processes wherein textile fibers are treated with strongly alkaline liquids. Examples of such processes arethe mercerization of cotton, the dyeing with vat dyestuffs, and the dyeing with sulfur dyestuifs. It is an object of my invention to so modify the treating bath or the textile fiber as to accelerate the time of the wetting of the fiber by the alkaline liquids and to render the penetration of the latter into the former more intense and more uniform.

It is already known to add special assisting agents to the mercerizing lyes which find application in the textile and artificial silk industry for the purpose of raising their wetting capacity and penetrating velocity. As such agents were proposed: lower alcohols, soap, Turkey red oils, aromatic sulfonic acids, as well as mixtures of cresol and benzyl alcohol or hydrophenols. Because of the tendency to be salted out in solid form on account of the highfelectrolyte content of the mercerizing lye (18 to"25% caustic soda) some of these agents such as soap, Turkey red oils and aromaticsulfonic acids are eitherusable for a short time only or not practical at all. Other agents become aggregated into large drops which float on top of the bath and interfere with the allimportant, uniform impregnation of the fibrous material w th the lye. Thesame, thing is true of the mixtures of benzyl alcohol with cresols diluents. I

I now found that practically infinitely stable dispersions, of a wetting capacity exceeding all known agents to an astonishing degree, may be obtained if into these mercerizing lyes are dispersed esters of higher fatty acids with lower alcohols such as methyl-oleate, ethyl-ricinate, methyl-stearate or esters of naphthenic acid with lower alcohols such as methyl-naphthenate, ethylnaphthenate, propyl-naphthenate.

in Germany March 14, 1930.

In practice, this method can be carried out I by emulsifying in a small portion of lye, and by the aid of vigorous stirring, a quantity of an ester selected from-the abovegroup corresponding to about 0.2 to 0.5 grams of the ester per liter of total mercerizing lye, and then adding this mixture to the main lye mass. Alternatively, the ester may be dissolved in a solvent which is miscible with at least one of the components of the -lye bath, that is one that is either water-soluble or alkali-soluble,- and this solution may then be added to the mercerizing lye. solvents may be mentioned lower-alcohols, ketones and esters on the one hand, andph'en01 and its homologues on the other hand. There are thus formed stable, highly disersed emulsions of the ester in the mercerlzing lye, which will instantly effect the sinking and shrinking of, say, cotton yarn or woven strips. I

Without limiting my invention, I submit herewith the following specific examples to illustrate the preferred modes of carrying out the same.

Ewemple 1 0.5 grams of methyl-oleate are emulsified in 10 cc..of caustic soda (28 B.) by the aid of a Turbo-agitator revolving at 2000 R. P. M., and this emulsion is added to 990 cc. of caustic soda 28 B. The lye thus obtained wets raw cotton instantly.

Ewample a? I 0.5 grams of naphthenic-acid-methyl-ester Ema/mple 3 0.5 grams of naphthenic-acid-methyl-ester are mixed with 4.5 grams of technical cresol and the mixture is added to 1 liter of 28 B. caustic soda. The lye thus obtained ex-- As such high wetting and penenaphthenic acids with lower alcohols in highly.dispersed form. As in the case of mercerizing lyes, the esters may be applied as such, or in solution in water-soluble or alkali-soluble organic solvents.

Example 4 To a dye vat containing 1 kilogram of thioindone-blue 3 .R, paste, (Colour Index, page 367), 840 grams of caustic soda 40 B.,

and 300 grams hydrosulfite concentrated powester dissolved in cc. of alcohol or dcr in 10 liters of water there is added with stirring 5 grams of naphthenic-acid-methylester dissolved in 50 grams of alcohol. When cotton is now introduced into the dye bath, it wets instantly.

in 1 liter of water there is added 0.5 gram of naphthenic-acid-ethyl-ester, dissolved in 5 cc. of alcohol. The vat obtained exhibits remarkably high wetting and penetrating powers.

Example 6 1 kg. naphthol AS (2,3-hydroxynaphthoic acid anilide) is pasted with 1.5 liters of caustic soda 34 B. into which has been incorporated 7.5 grams naphthenic-acid-methyL acetone, and this paste is dissolved in 15 liters-of hot water to a clear solution. This is then diluted by the addition of 15 liters of cold wets uniformly through water, 1 liter of formaldehyde 33% is added and the entire mass diluted to 300 liters. Cotton introduced into such a grounding bath in a very'shorttime.

Instead of adding the above assisting agents into the alkaline lye, they may be incorporated into the fibers, and the latter treated with the normal alkaline liquor in the ordinary'manner. The esters may be incorporated into the fibers as such, or after con-Y- version of the same into highly dispersed aqueous emulsions by the aid of known emulsifying agents.

Example 7' 1 kg. of raw cotton is uniformly impregnated with a solution of 5 grams of naphthenic-acid-methyl-ester in 200 grams acetone; the acetone is removed by evaporation and the yarn is introduced into a mercerizing lye of 28 B. It sinks instantly; the shrink- Example 8 By the aid of known emulsifyin agents, such as soaps, alkylated naphtha ene sulfonic acids, mineral oil sulfonic acids, and the like, a highly dispersed aqueous emulsion of 5 grams of naphthenic-acid-methyl-ester in 500 cc. is prepared and this is applied upon raw cotton yarn material by soakingor spraying. After drying, the material thus treated will wet instantly in a merceriz'ing lye, strongly alkaline vat, sulfur dye bath, (qr grounding bath for naphthol developing yes.

Other variations and modifications may be introduced in my novel processes above-de-' scribed, without departing from the spirit of my invention. 7

In the claims below it should be understood that by the term higher fatty acids I refer to acids which are derivable by hydrolysis of oils, fats, and waxes and which are illustrated by the following members: oleic, linoleic, stearic, palmitic, ricinoleic, lauric' and others. By the term lower monovalent alcohol I means the common lower alcohols, such as methyl, ethyl, propyl, butyl, amyl, or their lsomers.

I claim:

1. In the process of treating fibrous material with strongly alkaline liquors, the step of effecting said treatment in the presence of an ester selected from the group comprising esters of lower monovalent alcohols with unsulfonated higher fatty acids and esters of lower monovalent alcohols with unsulfonated naphthenic acids, whereby the wetting power and penetrating velocity of the alkaline liquors are increase 2. In the process of treating fibrous material with strongly alkaline liquors, the step of effecting said treatment in the presence of esters of lower monovalent alcohols with unsulfonated higher fatty acids whereby the wetting power and penetrating velocity of the alkaline liquors are increased.

3. In the process .of treating fibrous material with strongly alkaline liquors, the step of eifecting said treatment in the presence of esters of lower monovalent alcohols with unsulfonated naphthenic acids whereby the wetting power and penetrating velocity of the alkaline liquors are increased.

4. The process of improving the wetting powers of strongly alkaline treatment baths for fibrous materiahwhich comprises incorporating into such alkaline baths an ester 'selected from the group comprising esters of lower monovalent alcohols with unsulfonated higher fatty acids, and esters of lower monovalent alcohols with unsulfonated naphthenic acids.

5. The process of improving the wetting powers of alkaline treatment baths for fibrous material, which comprises incorporating into such alkaline baths esters of lower monovalent alcohols with unsulfonated higher fatty acids.

6. The process of improving the wetting powers of alkaline treatment baths for fibrous material, which comprises incorporating into such alkaline baths esters of lower monovalent alcohols with unsulfonated naphthenic acids.

7 In the process of treating' fibrous material with strongly alkaline liquors the step which comprises incorporating into fibrous material prior to the alkaline-bath treatment an ester selected from the group comprising esters of lower monovalent alcohols with unsulfonated higher fatty acids and esters of lower monovalent alcohols with unsulfonated naphthenic acids.

8. In the process of treating fibrous 'material with strongly alkaline liquors the step which comprises incorporating into fibrous material prior to the alkaline-bath treatment an ester of a lower monovalent alcohol with an unsulfonated higher fatty acid.

9. In the process of treating fibrous material with strongly alkaline liquors the step which comprises incorporating into fibrous material prior to the alkaline-bath treatment an ester of a lower monovalent alcohol with an unsulfonated naphthenic acid.

10. An alkaline treating bath for fibrous material containing an ester selected from a group comprising esters of lower monovalent alcohols with unsulfonated higher fatty acids and esters of lower monovalent alcohols with unsulfonated naphthenic acids.

11. An alkaline treating bath for fibrous material containing an ester of a lower monovalent alcohol with an unsulfonated higher fatty acid. p

12. An alkaline treating bath for fibrous material containing an ester of a lower monovalent alcohol with an unsulfonated naphthenic acid.

13. In the process of treating fibrousmaterial with strongly alkalne liquors, the step of effecting said treatm nt in the presence of an ester selected from the group consistmg of the methyl, ethyl or propyl esters of terial, the step unsulfonated oleic, ricinic, stearic and naphthenic acids, whereby the wetting power and pentrating velocity f the alkaline liquors are increased.

14. The process of improving the wetting powers of alkaline treatment baths for fibrous material, which comprises incorporating into such alkaline baths an ester selected from the group consisting of the methyl, ethyl or propylesters of unsulfonated oleic, ricinic,

stearic and naphthenic acids.

. 15. In the process of treating fibrous material with strongly alkaline liquors, the steps which comprises incorporating into fibrous material prior to the alkaline-bath treatment an ester selected from the group consising of the. methyl, ethyl or propyl esters of unsulfonated oleic, ricinic, stearic and naphthenic acids.

16. An alkaline treating bath for fibrous material containing an ester selected from the group consisting of the methyl, ethyl, or propyl esters of unsulfonated oleic, ricinic, stearic and naphthenic acids.

17. In' the process of mercerizing cotton material by. the aid of' strongly alkaline liquorsjthe step of effecting the mercerization in the presence of an ester selected from the group consisting of the methyl, ethyl, or propyl esters, of unsulfonated oleic, ricinic, stearic and naphthenic acids.

18. The process of improving the wetting powers of a mercerization-lye for cotton material, which comprises incorporating into such lye an ester selected from the group consisting of the methyl, ethyl, or propyl esters of unsulfonated oleic, ricinic, stearic and naphthenic acids.

19. In the process of mercerizing cottonmaing into said material prior to the mercerization treatment an ester selected from the group consisting of the methyl, ethyl, or

propyl esters of unsulfonated oleic, ricinic, stearic and naphthenic acids.

20.. A. mercerization bath for cotton material containing an ester selected from the group consisting of the methyl, ethyl, or

propyl esters of unsulfonated oleic, ricinic,

stearic and naphthenic acids.

I In testimony whereof, I have hereunto subscribed my name at Dresden, in the State of Saxony, Germany.

FRIEDRICH PosPrEoH.

which comprises incorporat- 

